Solidifying carbon dioxide



April 9, 1935. G. MAIURI I 1,997,151

SOLIDIFYING' CARBON DIOXIDE FiledOot.'l3, 1934 mvs/vrofi Go; DO MHIURI HTTOHNEI Patented Apr. 9, 1935 I UNITED STATES PATENT OFFlCE SOLIDIFYING CARBON DIOXIDE Guido Maiuri, fildwych, London, England, assignor to Maiuri Refrigeration Patents Limited, London, England Application October 13, 1934, Serial No. 748,155 In Great Britain October 24, 1933 5 Claims. (01. 62-121) g g i gg figif f g g a g i'g da td la ilailetifig however, to maintain the mould colder y1 car on 10x1 e, an is a e tom than at the top, which is required (oil ect 11).: to kgause carbon dioxide to be frozen into in order to produce solely condensation of carbon nse oc dioxide at the top and freezing of the liquid For the above purpose, according to the invencarbon dioxide at the bottom, it is necessary to 5 28:13:25??? dgxidezhistadilmtted tinto a. mould apply suction to the bottom of the coil to cause e a ve e rip e poin pressure and evaporation to take place there atthe lower temat a temperature above the liquefaction temperaperature. This will produce interruptions in the ture corresponding to the pressure, and the 111- area of the surface of the coil wetted by the rel0 :ernal surface 1tlhei mould isdmaintained at a fritgerant, with consequential serious interference empera ure w 10 ecreases ownwards along Wi h conduction of heat from the mould. Morethe internal surface of the mould from above to over with coils in parallel uniformity of flow bellow thg soliidificgtion tecfnrinlieragure th tlglough all the coils is rendered almost imposcar on 10x1 eisa e ino etopof si e. 15 a mould at a temperature above the liquefaction 0n the other hand continuity of the wetted 15 Iplomt and at" 1 ahpressiiure aibovefthe tipolle point surface and thereby heat conductivity can be essure, an e in erna sur ace 0 e wall preserve and uni orm cooling of a large numof the mould is maintained at a temperature less ber of moulds connected in parallel can be obthan that of liquefaction but at the top greater tained, by employing a flooded ys wherein than the solidification temperature, the carbon the l q d refrigerant is admitt d to th Cooling 20 dioxide W111 condense as dew on the surface of the l a e bottom d v porated by Suction grail of thetlllllollld 1and coalesce into1 drops and gpp t l p zl i u'fi a a e ent, ow own e sur ace an accumu a e at the W011 (1 Cause 8 m0 H1011 is to be bottom. If also the temperature of the wall of Colder at the 1501) than at the bottom Which is the mould at the bottom is below the solidificah contrary to wha is required. 25 tion temperature, the accumulating liquid carbon The above described disadvantages and difdioxide will.freeze into a dense block of ice, as ficult s are av d a Overcome y employing distinguished from iliIIOW. a mould, forbprodiilicing detnse solid carbon diox- By maintaining e pressure of the carbon ide from car on oxide a a pressure above the dioxide but slightly above the triple point pressure, triple p n W h is c l d by being di 30 the difierence between the liquefaction temperajacketed with a refrigeran in V r i ly interture and the solidification temperature can be rup Sections h of W h i pplied with kept small, for instance a maximum difierence refrigerant at the bottom and each of which is of the order of 5 to 6 C. Incidentally, th subjected to pressure reduction at the top, such solidification temperatureinsuch case willbe apthat h m n t m i of h Sect-i011 is 35 proximately the triple point temperature, that suitable to its situation on the mould and It is obviously essential that the mould b progressively lower than that of the section im-= colder at the bottom than at the top. This d ately above. v could be effected by cooling the mould indirectly Conveniently and preferably, the refrigerant ghrouglor a batlh ofnalco1l11ol, itself cgfiiled by rein each section of the jacket is not directly 40 rigera mg coi s. is owever wo invo ve a drawn off at the top of such section, but overtemperature d t or difference t flows into the bottom of the next section beg gfizl l rg gg g g 3 32 221 22;??? 3 :1? 2 33 1 neath, until it reaches the bottom section, from which it is directly drawn oil at the top. f g 9 tegllpoergturesvtlwolvedtfor By the above described superposed sectional ms aince 0 T f ure jacketing,'the advantage of good heat conducgradient of 6 to 8 C. 1s obviously ob ectionable tivit of a flooded 8 Stem of .acketin can be as it involves maintaining the cooling coils at d t J 1 g r te an excessively low temperature which is not only 0 mm W1 on e accompanymg Owe madditionally expensive but also difficult.

To avoid the temperature gradient involved by a hmdra'nce to workmg 1f indirect cooling f the mould through a bath, the height of each section of acket is kept such direct cooling of t mould by jacketing th that the difierence in temperature between top mould by a coil containing the evaporating reand bottom is small. frigerating agent can be adopted. Withsuch With, as is almost invariably the case in pracperature at the top than the bottom of each sec- 50 tice, jackets of moulds supplied with refrigerant in parallel, uniformity of flooding is ensured by interconnecting the bottoms of all the jacket sections of all the moulds at each level.

Each section of jacket is preferably separated from the adjoining section by a small vertical interval such that whilst the temperatures can be equalized by fiow of heat along the interven-. ing wall of the mould, there is little direct exchange of temperatures between sections.

'I'heheight of the top jacket section may exceed that of lower sections as a certain minimum total height is necessary to ensure an initial equal fiow of liquid refrigerant and equal cooling by the flooded system in a plurality of moulds connected in parallel.

A set of sectionally jacketed moulds as above described and of which only the front two are visible the remainder being thereby hidden, is illustrated in sectional elevation by way of example on the accompanying drawing, in which:

a are moulds, to which carbon dioxide gas at a pressure slightly above the triple point pressure is admitted at the top by a pipe b, branched to the several moulds, the branches of the pipe being individually provided with stop cocks 0. Alternatively, a single stop cock may be provided for a set of moulds.

The bottoms of the moulds a are closed by removable covers (1.

The wall of each mould is surrounded by three vertically separated jackets e e e Liquid refrigerant, such as liquid ammonia, is supplied by a pipe I, having a regulating valve 9, to branch pipes it connected to the bottom of each of the top jackets e Pipes i connect the tops of each of the top jackets e to the bottoms of the corresponding intermediate jackets 6 which also are interconnected at this level by pipes 7'. Similarly, pipes k connect the tops of each of the intermediate jackets e to the bottoms of the corresponding bottom jackets 6 which likewise are interconnected at this level by pipes l.

The tops of each bottom jacket e are interconnected by pipes m and all are connected by a pipe n to a region of extremely low subatmospheric pressure, such as a suitable absorber of an absorption refrigerating machine which supplies the liquid refrigerant by the above-mentioned pipe 1.

On starting or for testing, the moulds are vented of carbon dioxide gas by pipes o fitted with stop cocks p.

The liquid refrigerant floods the several jackets e e e and'also evaporates therein. As, however, the evaporation in the top jackets e and in the intermediate jackets e is effected against the static pressure head of the liquid refrigerant in the lower jacket or jackets e and e the evaporating pressures and therefore the mean temperatures in the jackets e will be higher than in the jackets e and higher in the jackets e than in the jackets e The temperature in the moulds a will therefore decrease from the top of the mould to the bottom.

The temperature of the moulds where surrounded by the top jackets e is arranged to be below the liquefying temperature of carbon dioxide at a pressure slightly above the triple point pressure, so that the carbon dioxide condenses there as dew on the walls of the'moulds and eventually flows down in drops. The temperatures in the moulds where surrounded by the jackets e and e is arranged to be below the sfiidification temperature of the carbon dioxide whereby the drops of liquid carbon dioxide collecting in this region become frozen into a block of ice q.

The intervals r between the'adjoining jackets e and e and e and e are suflicient to prevent direct exchange of temperatures between the jackets whilst being sufficiently narrow to prevent the mould becoming-hotter at these intervals.

In a representative example of working and construction, carbon dioxide gas is admitted to the top of each mould a at a pressure of 6 atmospheres absolute. A temperature of -56 C. is maintained at the bottom of each top jacket e two feet six inches in height, and a temperature of 58 C. at the top thereof, the mean temperature therefore being 5'7 C. In this upper part of the mould the heat transmission from the carbon dioxide condensing on the walls and fiowing down in liquid form is much higher than in the lower part, and for this reason a more energetic ebullition in the liquid refrigerant occurs, which causes a smaller drop of temperature relatively to the height than in the lower jackets. Each middle jacket e one foot six inches in height, has a temperature of 58 C. at the bottom and -60 C. at the top and a mean temperature of 59 C. Each bottom jacket e also one foot six inches in height, has a temperature of 60 C. at the bottom and 62 C. at the top and a mean temperature of 61 C.

The above temperatures can be obtained with jackets of the heights mentioned, if the jackets are filled with liquid ammonia of a density of 0.6 giving the required static pressure heads, and a suction pressure equal to 2000 m/m of water is applied to the outlet pipe n. This will give the temperature of 62 C. at the top of the jackets e The increase of pressure to 2300 m/m of water at the bottom of the jackets e will give the temperature of -60 C. At the bottom of the jackets e the pressure will be 2600 m/m of water and the temperature -58 C., and at the bottom of the jackets e the pressure will be 3000 m/m of water and the temperature 56 C.

The difference in temperature between the bottom and top of each jacket will become less if the amount of refrigerant vaporized is increased relatively to the volumetric capacity of each jacket, for instance by having jackets of narrow cross section, because in such case the formation of foam in each jacket will increase, thus reducing the static pressure head of liquid therein and the restraint to vaporization.

I claim:

1. A method of solidifying carbon dioxide consisting in admitting into a mduld carbon dioxide at a pressure slightly above the triple point pressure of carbon dioxide and at a temperature above the liquefaction temperature of carbon dioxide at said pressure, and maintaining the internal surface of said mould at a temperature which decreases downwards along said internal surface from above to below the solidification temperature of carbon dioxide at said pressure.

2. In a mould for the solidification of carbon dioxide, jackets embracing said mould at vertical intervals, means for supplying liquid refrigerant to the bottom of each of said jackets, and means for withdrawing refrigerant from the top of each of said jackets.

3. In a mould for the solidification of carbon dioxide, jackets embracing said mould at vertical intervals, means for supplying liquid refrigerant to the bottom of the topmost of said jackets,

means connecting the top oi each of said superposed jackets to the bottom of the jacket next beneath, and means for withdrawing refrigerant from the top of the lowermost of said jackets.

4. In a set of moulds for the solidification of carbon dioxide, jackets embracing each of said moulds at vertical intervals, means interconnecting the bottom of each of said jackets at each of said vertical intervals, means for supplying liquid refrigerant to the bottom of each of said jackets, and means for withdrawing refrigerant from the top of each of said jackets.

5. In a set of moulds for the solidification of carbon dioxide, jackets embracing each of said moulds at vertical intervals,'means interconnecting the bottom of each of said jackets at each of said vertical intervals, means for supplying liquid refrigerant to the bottom of the topmost of each of said jackets, means connecting the top of each of said superposed jackets to the bottom of the jacket next beneath, and means for withdrawing refrigerant from the top of the lower- 10 most of said jackets.

GUIDO MAIURI. 

